CN102976741B - Preparation method of manganese zinc MnZn soft magnetic ferrite material containing modified nanocarbon - Google Patents
Preparation method of manganese zinc MnZn soft magnetic ferrite material containing modified nanocarbon Download PDFInfo
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Abstract
The invention discloses a preparation method of manganese zinc MnZn soft magnetic ferrite material containing modified nanocarbon. The preparation method comprises the following steps of: preparing of main materials, preparing of auxiliary materials, presintering, mixing and secondary ball-milling of the main materials and the auxiliary materials, molding and sintering, and obtaining the MnZn soft magnetic ferrite material containing the modified nanocarbon. According to the preparation method of the manganese zinc MnZn soft magnetic ferrite material containing the modified nanocarbon. According to the invention, the added modified nanocarbon ingredients can serve as bridge conjugation among different raw materials, so that raw material distribution is better, and the manganese zinc MnZn soft magnetic ferrite material has the advantages of high density, high grain boundary resistivity, low porosity and big and uniform crystalline grain; the formulations of the raw materials are reasonably improved, and a magnetic core has higher magnetic conductivity after being sintered; and the indexes such as power loss, frequency characteristic, Curie temperature, saturated density and magnetic flux density and the like are all greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modified Nano carbon.
Background technology
High magnetic conductivity ferrite magnetic, magnetic core are to realize in the electronicss such as program control communication, digital technique, network communication colour TV, being used as the products such as inducer, wave filter, pulse transformer and making its miniaturization, the requisite electronic material of lightweight, improve constantly the initial permeability in magneticsubstance, be the pursuit of being engaged in these professional engineering technical personnel and production firm always.The history of traditional existing four more than ten years of conventional ceramic technique development high-permeability material for China, up to the present, can only reach 10000 left and right with the high-permeability material that conventional ceramic technique is produced, and the performance index of material are as all unsatisfactory in loss, frequency response characteristic, Curie temperature etc.
Summary of the invention
In order to alleviate shortcomings and deficiencies of the prior art, the object of the present invention is to provide a kind of preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modified Nano carbon.
The present invention adopts following technical scheme to achieve these goals:
The preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modified Nano carbon, comprises the following steps:
(1) join major ingredient: be Fe in molar ratio
2o
351-52mol, MnO 21-24mol, ZnO 24-27mol, V2O50.1-0.2mol prepare burden;
(2) join auxiliary material: be equivalent to the modified Nano carbon of major ingredient 0.01-0.02wt%, the lanthanum trioxide of 0.01-0.02wt%, the boron oxide of 0.04-0.05wt%, the ZrO of 0.02-0.03wt%
2cobalt oxide with 0.02-0.035wt%; Described modified Nano carbon is prepared by the following method:
A, trees ashes are soaked after 2-3 hour with the sodium hydroxide solution of 10-15%;
B, use 10-15% hydrochloric acid soln soak 2-3 hour;
C, with deionized water wash repeatedly, be neutral to trees ashes, dry;
D, be ground to 0.8-1.0 μ m powder, obtain modification trees ashes;
E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 3-5%, the nano silicon of 2-3%, be fully mixed to get;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 3-4 hour a time with dispersion agent, then spraying is dry, carries out pre-burning, and calcined temperature is 910-940 DEG C, and the pre-burning time is 1-2 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modified Nano carbon, add water and dispersion agent to carry out secondary ball milling 2-3 hour, spraying is dried, built in 200-250 order pellet;
(5) moulding: secondary ball abrasive material is mixed with modified Nano carbon, 12000-15000 rev/min, high speed dispersion 1-2 hour, is then pressed into base;
(6) sintering: put the moulded blank after above-mentioned moulding into sintering oven, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, be first warming up to 680-720 DEG C with 150-200 DEG C/h of speed, insulation 1-2 hour; In the nitrogen atmosphere of 0. 5%-1% oxygen volume content, while being warming up to 900 DEG C with 120-150 DEG C/h of speed, be incubated 0.5-1 hour; In the nitrogen atmosphere of 3%-5% oxygen volume content, then be warming up to 1280-1330 DEG C with 80-120 DEG C/h of speed, the sintered heat insulating time is 3-5 hour; After sintering, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, after cooling, obtain the MnZn magnetic ferrite magnetic core of modified Nano carbon.
Beneficial effect of the present invention:
1, the present invention, by adding modified Nano carbon component, can be used as the bridge keying action between different material, uses feed distribution better, density is high, grain boundary resistance rate is high, void content is low, crystal grain is large and even, rational modification composition of raw materials, after magnetic core is fired, has higher magnetic permeability;
2, there is higher DC superposition characteristic, solve the loose problem of magnetic core surface tissue, thereby the raising of product physical strength, magnetic permeability rising, loss are reduced;
3, the index such as power loss, frequency response characteristic, Curie temperature, saturation magnetic flux density all has greatly improved.
Embodiment
Embodiment 1: the preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modified Nano carbon, comprises the following steps:
(1) join major ingredient: be Fe in molar ratio
2o
351.5mol, MnO 22.35mol, ZnO 26mol, V2O50.15mol prepare burden;
(2) join auxiliary material: be equivalent to the modified Nano carbon of major ingredient 0.015wt%, the lanthanum trioxide of 0.015wt%, the boron oxide of 0.045wt%, the ZrO of 0.025wt%
2cobalt oxide with 0.028wt%; Described modified Nano carbon is prepared by the following method:
A, trees ashes are soaked after 2-3 hour with the sodium hydroxide solution of 10-15%;
B, use 10-15% hydrochloric acid soln soak 2-3 hour;
C, with deionized water wash repeatedly, be neutral to trees ashes, dry;
D, be ground to 0.8-1.0 μ m powder, obtain modification trees ashes;
E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 4%, 2.5% nano silicon, be fully mixed to get;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 3-4 hour a time with dispersion agent, then spraying is dry, carries out pre-burning, and calcined temperature is 925 DEG C, and the pre-burning time is 1-2 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modified Nano carbon, add water and dispersion agent to carry out secondary ball milling 2-3 hour, spraying is dried, built in 220 order pellets;
(5) moulding: secondary ball abrasive material is mixed with modified Nano carbon, and 13500 revs/min, high speed dispersion 1-2 hour, is then pressed into base;
(6) sintering: put the moulded blank after above-mentioned moulding into sintering oven, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, be first warming up to 700 DEG C with 180 DEG C/h of speed, insulation 1-2 hour; In the nitrogen atmosphere of 0.5%-1% oxygen volume content, while being warming up to 900 DEG C with 135 DEG C/h of speed, insulation 0.5-1 hour; In the nitrogen atmosphere of 3%-5% oxygen volume content, then be warming up to 1300 DEG C with 100 DEG C/h of speed, the sintered heat insulating time is 3-5 hour; After sintering, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, after cooling, obtain the MnZn magnetic ferrite magnetic core of modified Nano carbon.
The performance data of the magnetic ferrite magnetic core making by above-described embodiment:
Claims (1)
1. contain a preparation method for the manganese zinc (Mn-Zn) soft magnetic ferrite material of modified Nano carbon, it is characterized in that comprising the following steps:
(1) join major ingredient: be Fe in molar ratio
2o
351-52mol, MnO 21-24mol, ZnO 24-27mol, V
2o
50.1-0.2mol prepares burden;
(2) join auxiliary material: be equivalent to the modified Nano carbon of major ingredient 0.01-0.02wt%, the lanthanum trioxide of 0.01-0.02wt%, the boron oxide of 0.04-0.05wt%, the ZrO of 0.02-0.03wt%
2cobalt oxide with 0.02-0.035wt%; Described modified Nano carbon is prepared by the following method:
A, trees ashes are soaked after 2-3 hour with the sodium hydroxide solution of 10-15%;
B, use 10-15% hydrochloric acid soln soak 2-3 hour;
C, with deionized water wash repeatedly, be neutral to trees ashes, dry;
D, be ground to 0.8-1.0 μ m powder, obtain modification trees ashes;
E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 3-5%, the nano silicon of 2-3%, be fully mixed to get;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 3-4 hour a time with dispersion agent, then spraying is dry, carries out pre-burning, and calcined temperature is 910-940 DEG C, and the pre-burning time is 1-2 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modified Nano carbon, add water and dispersion agent to carry out secondary ball milling 2-3 hour, spraying is dried, built in 200-250 order pellet;
(5) moulding: secondary ball abrasive material is mixed with modified Nano carbon, 12000-15000 rev/min, high speed dispersion 1-2 hour, is then pressed into base;
(6) sintering: put the moulded blank after above-mentioned moulding into sintering oven, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, be first warming up to 680-720 DEG C with 150-200 DEG C/h of speed, insulation 1-2 hour; In the nitrogen atmosphere of 0. 5%-1% oxygen volume content, while being warming up to 900 DEG C with 120-150 DEG C/h of speed, be incubated 0.5-1 hour; In the nitrogen atmosphere of 3%-5% oxygen volume content, then be warming up to 1280-1330 DEG C with 80-120 DEG C/h of speed, the sintered heat insulating time is 3-5 hour; After sintering, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, after cooling, obtain the MnZn magnetic ferrite magnetic core of modified Nano carbon.
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Denomination of invention: A preparation method of Mn Zn MnZn soft magnetic ferrite containing modified nano carbon Effective date of registration: 20220525 Granted publication date: 20140611 Pledgee: Zhejiang Tailong Commercial Bank Co.,Ltd. Wenzhou Cangnan Qianku small and micro enterprise franchise sub branch Pledgor: Zhejiang Datong Magnetic Technology Co.,Ltd. Registration number: Y2022330000789 |
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